Method for preparing polychlorotrifluoroethylene resin

A polychlorotrifluoroethylene and resin technology, which is applied in the field of preparation of fluorine-containing polymer materials, can solve the problems of easy degradation, unstable end groups, low conversion rate of chlorotrifluoroethylene, etc., so as to improve the conversion rate and improve polymerization. The effect of reaction speed

Inactive Publication Date: 2012-07-25
CHANGSHU XINHUA CHEM
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  • Abstract
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  • Claims
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Problems solved by technology

[0005] PCTFE is polymerized from chlorotrifluoroethylene (CTFE) as a raw material. In order to obtain PCTFE with sufficient molecular weight to meet the needs of practical applications, a redox initiator system is usually used to polymerize at a lower temperature. The oxidant of the initiator system is generally It is persulfate or organic peroxide, and the reducing agent is sodium bisulfite and sodium metabisulfite. The actual polymerization reaction takes a long time, often exceeding 30 hours, and the conversion rate of chlorotrifluoroethylene is relatively low. The obtained PCTFE Despite its high molecular weight, there are unstable end groups on the molecular chain, which are easily degraded at...

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  • Method for preparing polychlorotrifluoroethylene resin
  • Method for preparing polychlorotrifluoroethylene resin

Examples

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Embodiment 1

[0033] In a 10-liter vertical SUS316L stainless steel polymerization reactor, add 5 kg of deionized water, 2 kg of perfluoro-4-methyl-2-pentane, 0.3 g of fluorine-containing decyl acrylate butanediol, 1.5 g of perfluoropentyl Butyl peroxide, control the stirring speed to 350 rpm, after deoxidation treatment, control the internal temperature of the polymerization tank to 40°C, add CTFE gas to make the internal pressure of the tank reach the gauge pressure of 0.9 MPa. When the pressure in the kettle drops to 0.8MPa, add CTFE gas to the kettle to maintain the pressure in the kettle at 0.85-0.9MPa. During the polymerization reaction, the internal temperature of the polymerization kettle was controlled at 40°C. When accumulatively 1.5 kilograms of CTFE monomers were added in the polymerization kettle, stop the feeding of CTFE, finish reaction after 1 hour. The total polymerization time was 8 hours. Recover the residual CTFE gas in the kettle, reduce the pressure of the kettle to ...

Embodiment 2

[0036] In a 10-liter vertical SUS316L stainless steel polymerization reactor, add 5.7 kg of deionized water, 1.3 kg of perfluoro-4-methyl-2-pentane, 0.35 g of fluorine-containing decanyl acrylate butanediol, and 1.4 g of perfluoropentyl Butyl peroxide, control the stirring speed to 350 rpm, after deoxidation treatment, control the internal temperature of the polymerization tank to 50°C, add CTFE gas to make the internal pressure of the tank reach the gauge pressure of 0.9 MPa. When the pressure in the kettle drops to 0.8MPa, add CTFE gas to the kettle to maintain the pressure in the kettle at 0.85-0.9MPa. During the polymerization reaction, the internal temperature of the polymerization kettle was controlled to 50°C. When accumulative 0.7 kilograms of CTFE monomers were added in the polymerization kettle, stop feeding of CTFE, finish reaction after 1 hour. The total polymerization time was 7 hours. The remaining CTFE gas in the kettle is recovered, the pressure of the kettle...

Embodiment 3

[0039] In a 10-liter vertical SUS316L stainless steel polymerization reactor, add 5 kg of deionized water, 2.5 kg of perfluoro-4-methyl-2-pentane, 5.625 g of fluorine-containing decanyl acrylate butanediol 9 g of perfluoropentyl Butyl peroxide, control the stirring speed to 350 rpm, after deoxidation treatment, control the inner temperature of the polymerization tank to 20°C, add CTFE gas to make the inner pressure of the tank reach the gauge pressure of 0.9 MPa. When the pressure in the kettle drops to 0.8MPa, add CTFE gas to the kettle to maintain the pressure in the kettle at 0.85-0.9MPa. During the polymerization reaction, the internal temperature of the polymerization kettle was controlled at 20°C. When accumulative 1.125 kilograms of CTFE monomers were added in the polymerization kettle, stop the feeding of CTFE, finish reaction after 1 hour. The total polymerization time was 6 hours. The remaining CTFE gas in the kettle is recovered, the pressure of the kettle is lowe...

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Abstract

The invention discloses a method for preparing polychlorotrifluoroethylene resin. The method includes: using CTFE (chlorotrifluor ethylene) as monomer, using mixture of deionized water with perfluor-4-methyl-2-pentane as media, and using perfluor-amyl-butyl peroxide initiator for polymerization of chlorotrifluoroethylene at the temperature of 0-70 DEG C in the existence of fluorine-contained decyl-acrylic acid dibutyl ester surfactant, wherein the feeding amount of the CTFE is 10-40 of the weight of the mixed media, the mass ratio of the deionized water to the perfluor-4-methyl-2-pentane is 2-5:1, usage of the perfluor-amyl-butyl peroxide initiator is 0.1-2% of the weight of CTFE, and usage of the fluorine-contained decyl-acrylic acid dibutyl ester surfactant is normally 0.02-2% of the weight of CTFE. The method is short in polymerization time and high in conversion rate, the obtained polymer is not easy to degrade, deteriorate in performance and discolor at high temperature.

Description

technical field [0001] The invention relates to a preparation method of polychlorotrifluoroethylene resin, belonging to the technical field of preparation of fluorine-containing polymer materials. Background technique [0002] PCTFE is a high value-added, high-performance thermoplastic. As a high-end product, it is often used in harsh environments where other materials cannot be used. When in contact with liquid oxygen, liquid nitrogen and liquefied natural gas, PCTFE has outstanding anti-brittle properties, excellent gas barrier characteristics, and is not affected by ultraviolet and gamma ray radiation. Among refrigerants, PCTFE has outstanding creep resistance characteristics, so it can be used for load bearing parts contacting refrigerant. [0003] PCTFE can be processed by common processes such as injection molding, extrusion, molding and transfer molding. PCTFE is mainly used to make parts of ultra-cold refrigeration equipment, valves (valve seats, valve stems, seal...

Claims

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Application Information

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IPC IPC(8): C08F114/24C08F4/34C08F2/00
Inventor 窦建华陶惠平徐卫
Owner CHANGSHU XINHUA CHEM
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